CN101275806A - Carbon dioxide supercritical drying device - Google Patents
Carbon dioxide supercritical drying device Download PDFInfo
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- CN101275806A CN101275806A CNA2007100648758A CN200710064875A CN101275806A CN 101275806 A CN101275806 A CN 101275806A CN A2007100648758 A CNA2007100648758 A CN A2007100648758A CN 200710064875 A CN200710064875 A CN 200710064875A CN 101275806 A CN101275806 A CN 101275806A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 55
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 55
- 238000000352 supercritical drying Methods 0.000 title claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
- 230000006837 decompression Effects 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000005057 refrigeration Methods 0.000 claims abstract description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 150000001298 alcohols Chemical class 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 210000004907 gland Anatomy 0.000 claims description 9
- 230000008676 import Effects 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 6
- 230000008016 vaporization Effects 0.000 claims description 6
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005459 micromachining Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000002309 gasification Methods 0.000 abstract 1
- 238000004377 microelectronic Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of sacrificial layer release of a key manufacturing technology of a micro electro mechanical system in a microelectronic technology, and discloses a carbon dioxide supercritical drying device, which comprises: the supercritical drying chamber is used for releasing the sacrificial layer and consists of a high-pressure reaction chamber 4 and a temperature control chamber 5; the high-pressure reaction chamber 4 is used for containing a silicon wafer support, providing a reaction chamber for carbon dioxide replacement and gasification drying and is connected with a carbon dioxide gas cylinder; the temperature control chamber 5 is connected with the high-pressure reaction chamber 4 through a coil pipe to realize refrigeration and heating of the high-pressure reaction chamber 4; and the separation decompression chamber 6 is connected with the high-pressure reaction chamber 4 through a pipeline and is used for separating the alcohols from the carbon dioxide and realizing decompression. The invention solves the problem of adhesion during drying in micro-machining, reduces the consumption of liquid carbon dioxide and achieves the aims of saving energy and reducing environmental pollution.
Description
Technical field
The present invention relates to the sacrifice layer release tech field of MEMS (MEMS) key manufacture in the microelectric technique, relate in particular to a kind of carbon dioxide supercritical drying device of freon refrigeration, when utilizing liquid CO 2 to enter supercriticality, carbon dioxide becomes and a kind ofly enters the characteristics of supercriticality like liquid like the surface tension that do not have of gas, solves the adhesion problems that wet processing occurs when dry.
Background technology
In MEMS (MEMS) manufacturing technology, the silicon substrate surface micromachining technology is an important component part, has avoided body silicon deep processing longitudinally, with integrated circuit technology better compatibility is arranged, and helps the integrated of structural devices and treatment circuit.
In silicon substrate surface micromachined process, " sacrifice layer " technology that apply to is made unsettled beam, film or cavity structure.In the sacrifice layer dispose procedure or after sacrifice layer forms, in most cases evaporating produces surface tension and causes that structure sheaf is drop-down, and this phenomenon is called adhesion phenomenon, and the CO 2 supercritical drier is to solve in the microfabrication adhesion the best way when dry.
Liquid under the supercriticality between the fine structure has just become a kind of capillary liquid (also can be called gas) that do not have, and carries out dry heat or decompression vaporization this moment again, the adhesion phenomenon that surface tension caused when the slow carburation by evaporation of liquid just can not take place.This equipment will obviously be better than additive methods such as freeze-dried method and organic displacement based on the effect of this principle.
The CO 2 supercritical drier uses in Japan-US MEMS scientific research now in a large number.But now domesticly entered breadboard this equipment and have only all one of Shanghai micro-system Americanized, and the equipment carbon dioxide-depleted amount of the U.S. is big, the carbon dioxide-depleted amount is at each three kilograms, and wherein 2/3rds are used for the chamber refrigeration, can cause the very big wasting of resources and air pollution.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention is to provide a kind of carbon dioxide supercritical drying device, solving in the microfabrication problem of adhesion when dry, and reduces the consumption of liquid CO 2, reaches the purpose of energy savings.
(2) technical scheme
For achieving the above object, technical scheme of the present invention is achieved in that
A kind of carbon dioxide supercritical drying device, this device comprises: supercritical drying chamber, be used for the release of sacrifice layer, form by reaction under high pressure chamber 4 and temperature-controlled chamber 5; Reaction under high pressure chamber 4 is used to hold the silicon chip support, and the reative cell of carbon dioxide replacement and vaporizing and drying is provided, and links to each other with dioxide bottle; Temperature-controlled chamber 5 links to each other with reaction under high pressure chamber 4 by coil pipe, realizes the refrigeration and the heating of reaction under high pressure chamber 4; Separation decompression chamber 6 links to each other with reaction under high pressure chamber 4 by pipeline, is used for alcohols and carbon dioxide separation, and realizes decompression.
4 tops, described reaction under high pressure chamber are equipped with high gland 1, are used for the sealed high pressure chamber.
Described high gland 1 is made by stainless steel material, and its diameter is 180mm, and height is 20mm.
Bottom, described reaction under high pressure chamber is equipped with import magnetic valve 401, outlet magnetic valve 403, temperature sensor 402, pressure sensor 404; Wherein, import magnetic valve 401 and outlet magnetic valve 403 are used to control the turnover of carbon dioxide; Temperature sensor 402 is used to test and control the temperature in the reaction under high pressure chamber 4; Pressure sensor 404 is used to test and control the pressure in the reaction under high pressure chamber 4.
Described reaction under high pressure chamber is the cylinder that stainless steel material is made, and its diameter is 135mm, and height is 82mm.
Described temperature-controlled chamber 5 is the freon refrigeration device, below reaction under high pressure chamber 4,4 links to each other in the reaction under high pressure chamber by coil pipe, and described silicon chip props up and is placed on 4 inside, reaction under high pressure chamber, and resistive heater directly posts the bottom in reaction under high pressure chamber 4.
Described separation decompression chamber is connected to air inlet pipe and decompression exhaust pipe 8, and air inlet pipe is used to connect reaction under high pressure chamber 4 and separation decompression chamber; Decompression exhaust pipe 8 is used to get rid of residual gas.
Described separation decompression chamber is the cylinder that stainless steel material is made, and its diameter is 135mm, and height is 200mm.
Described silicon chip support is diameter 120mm, the aluminium alloy cylinder of thickness 80mm, and above a diameter 105mm degree of depth is arranged is 2 millimeters concave station.
This device is moved automatically by relay temperature and pressure transmitter and valve control, and the safe self-locking function is set.
(3) beneficial effect
From technique scheme as can be seen, the present invention has following beneficial effect:
1, utilizes the present invention, the adhesion problems when adopting the CO 2 supercritical seasoning to solve the wet processing drying.Liquid under the supercriticality between the fine structure has just become a kind of capillary liquid (also can be called gas) that do not have, and carries out dry heat or decompression vaporization this moment again, the adhesion phenomenon that surface tension caused when the slow carburation by evaporation of liquid just can not take place.
2, utilize the present invention, adopt the mode of freon refrigeration, greatly reduce the consumption of liquid CO 2, saved the energy.
3, utilize the present invention, replace the carbon dioxide open refrigeration, consume great amount of carbon dioxide, the difficult problem of atmosphere pollution thereby overcome with the carbon dioxide open refrigeration with freon refrigeration.
4, utilize the present invention, increase the batch processing ability, four cun five batch processing ability of existing equipment is brought up to four cun ten batch processing ability, can single treatment ten four cun silicon chip, for industrialization is laid a good foundation.
5, utilize the present invention, adopt the pressure vessel that meets Chinese Industrial Standards (CIS), guaranteed the security of experiment.
6, utilize the present invention, in operation, with first manually back principle automatically, verify out optimum state after, the typing automation mechanized operation.And the equipment operation is carried out automatically by relay temperature and pressure transmitter and valve control, and the safe self-locking function is set.
Description of drawings
Fig. 1 is the schematic diagram of carbon dioxide supercritical drying device provided by the invention;
Fig. 2 is the structural representation of carbon dioxide supercritical drying device provided by the invention;
Fig. 3 is the schematic diagram of freon refrigeration in the carbon dioxide supercritical drying device provided by the invention;
Fig. 4 is the schematic diagram in carbon dioxide supercritical drying device mesohigh lid provided by the invention cross section;
Fig. 5 is the schematic diagram of carbon dioxide supercritical drying device mesohigh reative cell provided by the invention inside;
Fig. 6 is the schematic diagram of carbon dioxide supercritical drying device mesohigh reative cell provided by the invention bottom;
Fig. 7 is for holding the schematic diagram of the support of slice, thin piece in the carbon dioxide supercritical drying device provided by the invention;
Among the figure, high gland 1, a seat stand 2, hold the support 3 of slice, thin piece, reaction under high pressure chamber 4, temperature-controlled chamber 5, separation decompression chamber 6, carbon dioxide filter core 7, decompression exhaust pipe 8, freon compressore 9, evaporator coil 201, screw hole 301, import magnetic valve 401, temperature sensor 402, outlet magnetic valve 403, pressure sensor 404, gas cylinder 701, carbon dioxide air valve 702.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
As shown in Figure 1, Fig. 1 is the schematic diagram of carbon dioxide supercritical drying device provided by the invention.This device is made of two cylindric chambers, and two cylindric chambers are fixedly connected by a seat stand 2.Wherein, the cylindric chamber in left side is a supercritical drying chamber, is used for the release of sacrifice layer; The cylindric chamber on right side is a separation decompression chamber, is used for alcohols and carbon dioxide separation.
As shown in Figure 2, Fig. 2 is the structural representation of carbon dioxide supercritical drying device provided by the invention, and this device comprises supercritical drying chamber and separation decompression chamber 6.Wherein, supercritical drying chamber is used for the release of sacrifice layer, is made up of reaction under high pressure chamber 4 and temperature-controlled chamber 5.Reaction under high pressure chamber 4 is used to hold the silicon chip support, and the reative cell of carbon dioxide replacement and vaporizing and drying is provided, and links to each other with dioxide bottle.Temperature-controlled chamber 5 links to each other with reaction under high pressure chamber 4 by coil pipe, realizes the refrigeration and the heating of reaction under high pressure chamber 4.Separation decompression chamber 6 links to each other with reaction under high pressure chamber 4 by pipeline, is used for alcohols and carbon dioxide separation, and realizes decompression.
At the top of described reaction under high pressure chamber 4 high gland 1 is installed, is used for the sealed high pressure chamber.Described high gland 1 is made by stainless steel material, and its diameter is 180mm, and height is 20mm.As shown in Figure 4, Fig. 4 is the schematic diagram of carbon dioxide supercritical drying device mesohigh lid provided by the invention.
As shown in Figure 5 and Figure 6, Fig. 5 is the schematic diagram of carbon dioxide supercritical drying device mesohigh reative cell provided by the invention inside, and Fig. 6 is the schematic diagram of carbon dioxide supercritical drying device mesohigh reative cell provided by the invention bottom.Import magnetic valve 401, outlet magnetic valve 403, temperature sensor 402 and pressure sensor 404 are installed in the bottom of described reaction under high pressure chamber.Wherein, import magnetic valve 401 and outlet magnetic valve 403 are used to control the turnover of carbon dioxide; Temperature sensor 402 is used to test and control the temperature in the reaction under high pressure chamber 4; Pressure sensor 404 is used to test and control the pressure in the reaction under high pressure chamber 4.
Described reaction under high pressure chamber is the cylinder that stainless steel material is made, and its diameter is 135mm, and height is 82mm.During fabrication, adopt the pressure vessel that meets Chinese Industrial Standards (CIS), the MIL STD that the existing equipment of the U.S. adopts does not meet Chinese pressure criteria.The reaction under high pressure chamber that this equipment adopts is the cylinder of stainless steel material, diameter 135mm, high 82mm; High gland is also selected stainless steel material for use, diameter 180mm, high 20mm; Produced like this reaction under high pressure chamber meets Chinese Industrial Standards (CIS), has strengthened the security in the experiment.
Described temperature-controlled chamber 5 is the freon refrigeration device, below reaction under high pressure chamber 4,4 links to each other in the reaction under high pressure chamber by coil pipe, and described silicon chip props up and is placed on 4 inside, reaction under high pressure chamber, and resistive heater directly posts the bottom in reaction under high pressure chamber 4.
Compressor 9 in the freon refrigeration device passes through consumed power, freon after the vaporization is compressed into high temperature, high steam, and make the freon steam of this HTHP, flow through and be arranged on the evaporimeter of outside, hyperbaric chamber, just as the radiator heat radiation, to be dispersed in the outside air of hyperbaric chamber at the systemic heat in hyperbaric chamber, and make cold-producing medium become high temperature, highly pressurised liquid again, the freon as cold-producing medium just can recycle like this.Compressor constantly turns round, and the heat in the hyperbaric chamber will constantly be moved in the outer air of hyperbaric chamber and go, so just reached the purpose of refrigeration.Specifically as shown in Figure 3, Fig. 3 is the schematic diagram of freon refrigeration in the carbon dioxide supercritical drying device provided by the invention.
Described separation decompression chamber is connected to air inlet pipe and decompression exhaust pipe 8, and air inlet pipe is used to connect reaction under high pressure chamber 4 and separation decompression chamber; Decompression exhaust pipe 8 is used to get rid of residual gas.
Described separation decompression chamber is the cylinder that stainless steel material is made, and its diameter is 135mm, and height is 200mm.
As shown in Figure 7, Fig. 7 is for holding the schematic diagram of the support of slice, thin piece in the carbon dioxide supercritical drying device provided by the invention.Described silicon chip support is diameter 120mm, the aluminium alloy cylinder of thickness 80mm, and above a diameter 105mm degree of depth is arranged is 2 millimeters concave station.
This device is moved automatically by relay temperature and pressure transmitter and valve control, and the safe self-locking function is set.
Dioxide bottle links to each other with supercritical drying chamber by air valve, and air valve is used to control the break-make of gas; The freon refrigeration device is below the hyperbaric chamber, by coil pipe continuous realization temperature control in the reaction under high pressure chamber; Supercritical drying chamber links to each other with separation decompression chamber by pipeline and realizes the purpose of displacement alcohols and decompression.
In use, open high gland 1 earlier, sheet submounts 3 is put into reaction under high pressure chamber 4, drive main power source, panel power supply, manually opened carbon dioxide air valve, record gas cylinder weight, and the residual amount of estimation liquid gas.Begin cooling then, whole reaction under high pressure chamber 4 temperature are down to zero by freon refrigeration, temperature sensor 402 starts import magnetic valve 401 to reaction under high pressure chamber 4 feed liquor attitude carbon dioxide after arriving zero degree, when reaction under high pressure chamber 4 internal pressures reach 4MPa, stop automatically flowing, after about 5 minutes, open reaction under high pressure chamber outlet magnetic valve 403, begin to replace the alcohols in the reaction under high pressure chamber 4, make it flow into separation decompression chamber 6, the time controlled relay pick up counting.Close outlet magnetic valve 403 after 30 minutes.Also close simultaneously import magnetic valve 401 after 5 minutes.Begin heating, temperature to 36 degree stops heating, and keeps a period of time, and after 5 minutes, pressure reaches 73MPa, opens the outlet magnetic valve.Pressure decline liquid carbon dioxide all gasifies, and dry run is finished.Close gas cylinder valve, the operating desk outage, primary power source de-energizes is cleaned stainless steel and is crossed filter core, fills in service recorder.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a carbon dioxide supercritical drying device is characterized in that, this device comprises:
Supercritical drying chamber is used for the release of sacrifice layer, is made up of reaction under high pressure chamber (4) and temperature-controlled chamber (5); Reaction under high pressure chamber (4) is used to hold the silicon chip support, and the reative cell of carbon dioxide replacement and vaporizing and drying is provided, and links to each other with dioxide bottle; Temperature-controlled chamber (5) links to each other with reaction under high pressure chamber (4) by coil pipe, realizes the refrigeration and the heating of reaction under high pressure chamber (4);
Separation decompression chamber (6) links to each other with reaction under high pressure chamber (4) by pipeline, is used for alcohols and carbon dioxide separation, and realizes decompression.
2. carbon dioxide supercritical drying device according to claim 1 is characterized in that, top, described reaction under high pressure chamber (4) is equipped with high gland (1), is used for the sealed high pressure chamber.
3. carbon dioxide supercritical drying device according to claim 2 is characterized in that, described high gland (1) is made by stainless steel material, and its diameter is 180mm, and height is 20mm.
4. carbon dioxide supercritical drying device according to claim 1 is characterized in that, bottom, described reaction under high pressure chamber is equipped with import magnetic valve (401), outlet magnetic valve (403), temperature sensor (402), pressure sensor (404); Wherein, import magnetic valve (401) and outlet magnetic valve (403) are used to control the turnover of carbon dioxide; Temperature sensor (402) is used for the temperature in test and the control reaction under high pressure chamber (4); Pressure sensor (404) is used for the pressure in test and the control reaction under high pressure chamber (4).
5. carbon dioxide supercritical drying device according to claim 1 is characterized in that, described reaction under high pressure chamber is the cylinder that stainless steel material is made, and its diameter is 135mm, and height is 82mm.
6. carbon dioxide supercritical drying device according to claim 1, it is characterized in that, described temperature-controlled chamber (5) is the freon refrigeration device, below reaction under high pressure chamber (4), link to each other in reaction under high pressure chamber (4) by coil pipe, described silicon chip props up and is placed on inside, reaction under high pressure chamber (4), and resistive heater directly posts the bottom in reaction under high pressure chamber (4).
7. carbon dioxide supercritical drying device according to claim 1 is characterized in that, described separation decompression chamber is connected to air inlet pipe and decompression exhaust pipe (8), and air inlet pipe is used to connect reaction under high pressure chamber (4) and separation decompression chamber; Decompression exhaust pipe (8) is used to get rid of residual gas.
8. according to claim 1 or 7 described carbon dioxide supercritical drying devices, it is characterized in that described separation decompression chamber is the cylinder that stainless steel material is made, its diameter is 135mm, and height is 200mm.
9. carbon dioxide supercritical drying device according to claim 1 is characterized in that, described silicon chip support is diameter 120mm, the aluminium alloy cylinder of thickness 80mm, and above a diameter 105mm degree of depth is arranged is 2 millimeters concave station.
10. carbon dioxide supercritical drying device according to claim 1 is characterized in that, this device is moved automatically by relay temperature and pressure transmitter and valve control, and the safe self-locking function is set.
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CNA2007100648758A CN101275806A (en) | 2007-03-28 | 2007-03-28 | Carbon dioxide supercritical drying device |
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CNA2007100648758A CN101275806A (en) | 2007-03-28 | 2007-03-28 | Carbon dioxide supercritical drying device |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101740342B (en) * | 2008-11-26 | 2011-08-31 | 中国科学院微电子研究所 | Carbon dioxide supercritical fluid semiconductor cleaning equipment |
CN101433562B (en) * | 2008-12-17 | 2011-09-07 | 中国林业科学研究院林产化学工业研究所 | Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof |
CN102345968A (en) * | 2010-07-30 | 2012-02-08 | 中国科学院微电子研究所 | Device and method for drying microemulsion based on supercritical carbon dioxide |
CN113432387A (en) * | 2021-08-02 | 2021-09-24 | 贵州航天乌江机电设备有限责任公司 | Supercritical carbon dioxide drying device for aerogel glass |
CN116272748A (en) * | 2023-04-25 | 2023-06-23 | 清华大学 | System and method for supercritical thermal degradation of refrigerants |
-
2007
- 2007-03-28 CN CNA2007100648758A patent/CN101275806A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101740342B (en) * | 2008-11-26 | 2011-08-31 | 中国科学院微电子研究所 | Carbon dioxide supercritical fluid semiconductor cleaning equipment |
CN101433562B (en) * | 2008-12-17 | 2011-09-07 | 中国林业科学研究院林产化学工业研究所 | Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof |
CN102345968A (en) * | 2010-07-30 | 2012-02-08 | 中国科学院微电子研究所 | Device and method for drying microemulsion based on supercritical carbon dioxide |
CN102345968B (en) * | 2010-07-30 | 2013-07-31 | 中国科学院微电子研究所 | Device and method for drying microemulsion based on supercritical carbon dioxide |
CN113432387A (en) * | 2021-08-02 | 2021-09-24 | 贵州航天乌江机电设备有限责任公司 | Supercritical carbon dioxide drying device for aerogel glass |
CN113432387B (en) * | 2021-08-02 | 2024-04-30 | 贵州航天乌江机电设备有限责任公司 | Supercritical carbon dioxide drying device for aerogel glass |
CN116272748A (en) * | 2023-04-25 | 2023-06-23 | 清华大学 | System and method for supercritical thermal degradation of refrigerants |
CN116272748B (en) * | 2023-04-25 | 2024-02-06 | 清华大学 | System and method for supercritical thermal degradation of refrigerants |
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